Henry v



PatentedIAug; 255 h g H I U ITED STATES PATENT OFFICE.

Emu? nuNnm,-or norm venues, new roux.

'--iilomrrr.ncasam Am) rnocrss or MAKING sum.

. This process has'forits object the manu- 2o: casein 1s s) ,facture of a novel casein product well suited for use in sizing and finishing paper, leather and cloth, when a low-viscosity dissolve-d ,sizing. is jdesired-.' The "product is also of value as the starting pointfor the manu-" facture'of medicinal products because of its "peculiar properties, some of which are here- I 1ndescribed.

V When casein is dissolved, with a-considerable excess of sodium or potassium hydroxide, in water, with the aid ,of heat, a portion of the nitrogen content of the broken down forming ammonia.

at the same time the casein solution begins to change in color to a light yellow and "later-to a yellowish brown solution. .During reduced in viscosity and finally becomes a very thin solution depositing .or throwing this treatment the casein solution is [out of solution a softfopaque white-precipitate which may amountto about 6 to 10% 0:

of the weight of the; original casein. If, after the above mentioned reaction has taken place tot-he desired degree, an ammonium salt,;such"as ammonium chloride is added in suflicient amount to-reactiwi t excess of caustic alkali present, there will be formed from the" excess oflTaOI I,,ainmoprocess, I give .cedure which isby ro ortions of NaOI-I and there-'- rub acidity may" be neutral, slightly acid, "or slightly alin the casein mixture.

'fore of depending u nium hydroxideand-common salt. By boilingthe mixture,-- o r by drying the casein product, the-ammonia is expelled from the product. This casein product when finished;

on the amount or kaline, depending i u v 'zethe caustic alkali NILCI used to neutra more clearly. describe this below an example of proway of illustration only,

In order to since the l can-be varied-considerably, o'n-the grade or quality of casein used an the alkalinity, neutrality or of the product desired. ;To 100 pounds of casein I add '300,pounds' of water and 15 poundsof caustic soda. This represents a considerable excess of the latter.

"stroy' the extreme the caustic alkali a er it has acte upon the].

salts may oxalate, persulfate, tungstate 0r fluorides Application flied larch 22, 1923 Serial No. 626,981.

These are well"mixed together and heated to about 170 F. The mixture is now al-- lowed to stand, with occasional stirring,

for about three hours or longer. I then'add .15 pounds of ammonium chloride, -which' has been dissolved in alittle water, in order to neutralize or change over all or nearly all of thefree NaOH remaining. Thc'mixture is then boiled or well heated again and tested for. freeNaOH. If any is found, more ammonium chloride is added, little by little, until the mixture is neutral, or one may, if desired, leave the'solution slightly alkaline by leaving a portion of the NaOI-I unchan ed. In any case, when the desired alkalinity or neutrality is secured, the solution may be further concentrated by evaporation in any of the well known evaporators or it may be completely dried. good methodfor making it into a dry powder is to dry the solution on. a so-called Just milk drying machine. The resulting powder may be sifted when it is ready, for use.

About yield can be secured, based on the amount of casein used,

In this example, the liquid was not -filsuch filtration is not precluded, and may even be advantageous if a roduct is wanted which will-give an entire y clear solution. In place of'ammonium chloride, I may use 0t free caustic alkali l alkaline pro ertiesof casein, without precipitating the casein or the greater portion thereof, as would be the 'tered before the drying operation, although er ammonium salts to react with the the object being to de-' caseif. strong. acids were to be used. For

example, I-ma use ammonium sulfate in place of the ch oride'or if I des'irean alkaline product(but not caustic) ,"I may use ammonium phosphate or other ammonium be used, such as the carbonate,

*L'If this product is dissolved ,by meansof a solvent commonly .used to dissolve casein, for example borax, and the resulting solution precipitated with an acid, for ex- \ample, by hydrochloric acid, only from to of the original weight of the.-.casem same conditions the entire amount'would be preci itated.

2. f the modified casein is mixed with cold water, for examlpile one. part modified water an apparently casein with 4 parts co opa no solution is the result. However, on heating this solution, about is precipitated or thrown out, leaving the balance of the material as a water clear solution. This latter solution is not precipitated by alkalies or acids. An analysis of the dried residue of this solution shows nitrogen 10.57% and ash about 8 j 3.. If ferric chloride is added to that last mentioned clear solution under 2, there is a precipitate formed amounting to about 37% on the basis of the dry modified casein used. This product, when dry, shows an analysis 11.55% nitrogen, 8.16% ash (including 4.56% ferric oxide). The product is entirely soluble in 1%solution of hydrochloric acld.

dissolve the same, heating same sufliciently 'to liberate a portion of the nitrogen content of the casein in the form of ammonia, and thereafter neutralizing at least a large part of the remaining caustic alkali with an ammonium salt.

2. A process which comprises adding to casein material, with water, a caustic alkali in substantial excess over the amount necessary to dissolve the same, allowin the alkali to act until the viscosity .is o y a small fraction of the normal viscosity of a solution of undecomplosed casein in mild alkali and containing t e same amount of casein, showing the formation ofa chemically modified casein, adding an ammonium salt in amount 'or part at least of the casein material, with water,- a caustic a ali V in substantial excess ov'er the amount necessary to dissolve the same, allowing the alkali and containing the same amount of casein,

showing the formation of a chemically modified casein, adding-an ammonium salt and thereafter drying the liquid.

4. A process which comprises adding to casein mater al, with water, a caustic alkali in substantial excess over the amount necessary to dissolve the same, allowing the alkali to act until the viscosity is only-a small fraction of the normal viscosity of a solution of undecomposed casein in mild alkali and containing the same amount of casein, showing the formation of a chemically modified casein, addin a salt of a volatile base and heating sufiiciently to drive ofi volatile base.

5. A process which comprises adding water and an excess of caustic alkali to casein and heatin sufliciently to form ammonia, and therea r neutrahzing excess alkali with an ammonium compound.

6. A modified casein product, which, when dissolved in an ordinary casein solvent and acidified will throw down a precipitate amounting to only about half the uantity of the original casein, such modifie casein product forming an apparent solution with cold water, which solution when boiled will throw down a precigitate equal in amount to about a third of t e original casein, leaving a clear solution of a'materi containing about 10.5% N.

In testimony whereof I aflix my signature. 

